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( 12 ) United States Patent US010132144B2 (12 ) United States Patent ( 10 ) Patent No. : US 10 , 132 , 144 B2 Lawson et al. ( 45 ) Date of Patent : Nov . 20 , 2018 ( 54 ) GEOCHEMICAL METHODS FOR ( 58 ) Field of Classification Search MONITORING AND EVALUATING CPC .. CO9K 8 / 58 ; CO9K 8 /582 ; CO9K 8 / 90 ; E21B MICROBIAL ENHANCED RECOVERY 43 / 16 OPERATIONS See application file for complete search history . (71 ) Applicants :Michael Lawson , Spring , TX (US ) ; Amelia C . Robinson , Houston , TX (56 ) References Cited (US ) ; Daniel A . Stolper , Berkeley , CA U . S . PATENT DOCUMENTS (US ) 4 , 833 , 915 A 5 / 1989 Radd et al . (72 ) Inventors : Michael Lawson , Spring , TX (US ); 4 , 905 ,761 A 3 / 1990 Bryant Amelia C . Robinson , Houston , TX ( Continued ) (US ) ; Daniel A . Stolper, Berkeley, CA (US ) FOREIGN PATENT DOCUMENTS CN 102154453 A 8 / 2011 ( 73) Assignee : ExxonMobil Upstream Research WO WO 2002 /059351 A2 8 / 2002 Company , Spring , TX (US ) ( Continued ) ( * ) Notice : Subject to any disclaimer, the term of this patent is extended or adjusted under 35 OTHER PUBLICATIONS U . S . C . 154 ( b ) by 0 days. Chung et al. ( 1988) " Origin of gaseous hydrocarbons in subsurface (21 ) Appl . No. : 15 /668 , 395 environments : theoretical considerations of carbon isotope distri bution ” , Chemical Geology , vol. 71 , pp . 97 - 103 . (22 ) Filed : Aug. 3 , 2017 (Continued ) (65 ) Prior Publication Data Primary Examiner — Zakiya W Bates US 2018 /0066504 A1 Mar . 8 , 2018 Assistant Examiner — Crystal J Miller (74 ) Attorney, Agent, or Firm — Exxonmobil Upstream Related U . S . Application Data Research Company Law Department ( 60 ) Provisional application No . 62 /382 , 921 , filed on Sep . 2 , 2016 . (57 ) ABSTRACT Described herein are methods and techniques that utilize ( 51 ) Int. Ci. molecular geochemistry and isotopic signatures to monitor E21B 43 / 16 ( 2006 . 01 ) microbial enhanced gas and oil recovery operations. The CO9K 8 /582 ( 2006 .01 ) methods and techniques utilize multiply substituted isoto (Continued ) pologue signatures, clumped isotope signatures , and /or posi (52 ) U . S . CI. tion - specific isotope signatures of one or more byproducts of CPC .. .. .. .. E21B 43 / 16 ( 2013 .01 ) ; C09K 8 /582 the microbial stimulation techniques to determine the effec ( 2013 .01 ) ; C09K 8 / 90 (2013 . 01 ) ; E21B 43/ 25 tiveness of a microbial stimulation technique . ( 2013 . 01 ) ; (Continued ) 18 Claims, 2 Drawing Sheets Collect sample from producing weil to characterizeisotopic the naturalsignature background Slimulate the well using microbial stimulation techniques Collect sample turn the stimulated well to characterize the induced isotopic signature 108 Analyze the clifferences between the induced isotopic signature and the background isotopic signature 110 Optionally , collcct samples for the Stimulated well over a period of time to characterize the induced isotopic www. signanire over time . 112 Optionally , analyze the differences in the induced isotopic signature over tinc 114 Develop or refine stimulation strategy trased on the inducecl isotopic signalLiTV - 116 Produce hydrocarbons US 10 ,132 ,144 B2 Page 2 ( 51) Int . CI. 2015 / 0240633 A1 * 8 / 2015 Akkurt .. .. .. E21B 49 /088 CO9K 8 / 90 175 / 50 ( 2006 .01 ) 2015 /0284810 Al 10 /2015 Knight et al . E21B 43 / 25 ( 2006 .01 ) 2015 /0291992 Al 10 /2015 Al-Moniee et al . GOIN 33 / 28 ( 2006 . 01 ) 2016 / 0018558 A1 * 1 / 2016 Bond GOIV 8 / 02 GOIV 9 /00 ( 2006 . 01) 250 / 255 C12P 1 /00 2016 / 0084045 Al 3 / 2016 Lawson et al. ( 2006 .01 ) 2016 /0084080 A1 3 / 2016 Lawson et al. C12P 39 / 00 (2006 .01 ) 2016 / 0084081 Al 3 / 2016 Lawson et al. U . S . Ci. 2016 / 0084817 A1 3 / 2016 Lawson et al. 2016 /0222781 A18 / 2016 Lawson et al . CPC . .. .. GOIN 33 /2823 (2013 . 01 ) ; GOIV 9 /007 2016 /0222782 A1 * 8 /2016 Lawson . .. .. .. .. .. GOIN 33 / 241 ( 2013. 01 ) ; C12P 1 / 00 ( 2013 .01 ); C12P 39 /00 2016 / 0258922 A1 * 9 / 2016 Formolo . .. .. .. .. .. E21B 49 / 00 (2013 .01 ) 2016 /0272962 AL 9 /2016 Kohr 2016 /0341038 A1 * 11/ 2016 AbuAli .. GOIN 1 / 2294 ( 56 ) References Cited U . S . 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